Process for the batch distillation of liquid mixtures



- y 1939. w. J. D. VAN DIJCK 5 2 PROCESS FOR THE BATCH DISTILIJATION OF LIQUID MIXTURES Filed March 8, 1937 I1 1] I J 1o 7H1 WVWWW -lNVENTOR-WlLLEM JOHAN E5 DOMINICUS VAN DUCK 2w HIS ATTORNEY Patented May 23, 1939 I v UNITED STATES PATENT OFFICE PROCESS FOR THE BATCH DISTILLATION OF LIQUID MIXTURES Willem Johannes Dominicus van Dijck, The

- Hague, Netherlands, assignor to Shell Development Company, San Francisco, Calif., a corporation of Delaware Application March 8, 1937, Serial No. 129,564

In the Netherlands March 12, 1936 3 Claims. (Cl. 202-39) The invention relates to a process and appaoriginal stock (present in one'or more tanksi'o'r ratus for the batch distillation of liquid mixto one or more other storage tanks. tures. Further according to the invention a heat ex- The fractionating of liquid mixtures, such as change is efiected between the mixture flowing 6 those of the nature of mineral oil or mineral oil from storage to the distillation zone andthe mixproducts, is nowadays practically always effected ture drawn off from the distillation zone. It is continuously. When, however, it is desired to thus attained that the temperature of the'mixproduce continuouslyalarge number of relatively. ture outside the distillation zone does not benarrow fractions, 1. e., fractions having a narrow come high, so that the respective storage tank 10 boiling range, any two successive ones of which or tanks need not be constructed for high temper- 10 do not or only slightly overlap, a complicated atures. i and costly apparatus with many columns is re- The quantity of liquid flowing to the distillaquired. If moreover the composition of the inition zone per unit of time naturally exceeds the tial material does not remain quite constant, such quantity flowing in opposite direction, although an apparatus is very diflicult to control in view of the said quantity may be of the order of the 15 the regulation of any one column affecting all quantity of liquid fed. In fact, the former quane the subsequent columns. tity is the sum of the circulating quantity and When applying the usual batch process it is the top and bottom products. Consequently a indeed possible to produce a large number of narlarger quantity of cold than of hot liquid flows row fractions with a simpler apparatus, the conthrough the heat-exchanger, which increases its 20 trolbeing then also much simpler in view of the efficiency. The pumps by means of which the various. fractions appearing in succession, but liquid is forced from and to the distillation zone such a process requires much heat. Moreover are, according to the invention, preferably couthis batch process involves several other drawpled mechanically, such with a view to a proper backs, to which further reference will be made control, this mechanical coupling being of par- 25 later on, and one of which is very obvious, viz., ticular importance when a superatmospheric the drawback-at least if it is desired to keep the pressure or a vacuum is maintained in the distildimensions of the stills, etc., within reasonable lation zone. The said pumps are further preflimits-that only relatively small charges can be erably placed at the cold end of the heat-exworked at a time, so that much time and labour changer. 30 is involved in the refilling of the stills, the heat- The distillation zone may, for example, com ing and adjusting of the apparatus, the changsist of a column known per so from the continuing-over to other distillate receiving tanks and ous distillation, which is heated at the bottom, the mixing of the fractions of the same composie. g., by circulating a portion of'the bottom prodtion obtained in the successive distillations. not and heating it outside the column. Further 35 Now the invention relates to a method accordthe column maybe equipped with the usual trays ing to which the distillation is also carried out with bubble caps or other means for effecting a discontinuously, but whereby the above-menthorough contact and a good exchange between tioned drawbacks are avoided. By batch distilvapour and liquid. At the top of the column the 40 lation (discontinuous distillation) is meant here vapours are withdrawn, a portion thereof after 40 a method of distilling whereby the.composition condensation being ret s reflux t0 the top or the products formed changes with time, i. e., of e c The e vy ro u t is awn f substantially no extraneous distillable liquid is in the hquid state 0m the bottom. of the introduced into the distillation system compris- The liquid flowing top to bottom is 5 ing t e storage tank and the distillation column withdrawn from the column Just above the feed m the course of the distillation and pumped to the original storage tank or a secd storage tank whilst it is not essential that According to the invention the liquid mixture :3 the H i quid flowing down Is withdrawn. A porto be distilled is fed continuously from a storage tion may flow ofi in the usual manner to the feed gfg i g g g tfigfif i fgig $3213 3; tray, which may sometimes be of advantage with 50 a view to facilitating the control. The mixture simultaneously separated off, while intermediate already ubje ted t distillation, which is mixture is continuously drawn off from the (he tinuously drawn off from the distillation zone, tillation zone. The latter mixture may, accordgenerally diff rs in composition from the reflux 65 in to the invention. be returned either to the returned into the column at the top.

The process according to the invention is explained below with reference to the drawing.

The storage tank I contains the liquid to be distilled, e. g., a crude benzine. By means of the pump 3 the oil is forced from the tank through conduit 2 and heat-echanger 4 to the middle of column 5. Column 5 is provided with a reboiler 6, in which a portion of the bottom product is heated and from which it is returned to the bottom of the column. At the top of the column theyapours of the light product escape through conduit l3; these vapours are condensed in condenser l and a portion of the condensate is returned as reflux into the column through conduit 8. The top product is drawn ofi through conduit 9 and-in so far as necessary-further condensed, 'if desired, in several steps to effect a fractionation.

The bottom product is withdrawn at the bottom of the column through conduit l2. The liquid flowing down in the column is returned to storage tank I through conduit l0 and heat-exchanger 4, by means of pump H. The reflux returned to the storage tank is mixed with the feed liquid therein. If the mixing of the two liquids is not desired, care must be exercised to avoid agitation when discharging the reflux into tank I, or a separate tank may be provided for receiving the withdrawn reflux.

When the apparatus dutlined above is put into operation, the lightest fraction is drawn off as top product at the top of the column and the heaviest fraction as bottom product at the bot tom of the column. As the distillation proceeds the composition of the top product becomes heavier and that of the bottom product lighter, so that any number of light fractions with increasing specific gravity or boiling point and at the same time any number of heavy fractions with decreasing specific gravity or boiling point may be collected, until finally the compositions of top and bottom product become substantially the same, when the distillation has been completed, whilst the product still present in the storage tank is drawn off as a pure fraction. A new charge can then be treated.

The manner of supplying heat to the column by means of reboiler 6, as described, is not the only one possible. Besides this or instead thereof boilers or other plants known per se may be used for supplying the heat required. Further a storage tank may be connected up to more than one column or one column to more than one storage tank. One may, for example, proceed in such amanner that while the contents of one or several tanks are being distilled, another tank or several other tanks are being filled with a new charge. The distillation may, for example, also be carried out in one column until the liquid in the storage tank has acquired a certain composition, after which the distillation may be continued in anothercolumn.

As the method described will be applied in particular to obtain a number of narrow fractions, one may, for instance, after these fractions have been obtained, distil the remainderif no narrow fractions are required-further in a conventional continuous manner.

The process according to the invention offers various important advantages as compared with conventional batch distillation. Since a top product and a bottom product are manufactured simultaneously, the consumption of heat is only half that which would be required if the same fractions were to be produced according to the known batch distillation.

The storage tank(s) may be very large in relation to the size of the column. It is, therefore, possible to work very large charges at a time, so that the compositions of top product and bottom product change relatively slowly; which is of advantage for an easy control of the apparatus, since only when the, column runs through a series of pseudo equilibria can its maximum efflciency be achieved.

No large stills being present, in which the liquid is to be kept at a high temperature for a considerable time-as is the case with the usual batch distillation-the danger of thermal decomposition isreduced to a minimum.

One may also dispense with heating the stock to the boiling point, during which period no products are obtained, much time and labour thus being saved.

Finally the existing continuous distilling plants may be adapted in a simple manner to carrying out the process according to the invention, since any normal continuous process-column can be used for this purpose. The process according to the invention may in principle be applied to any liquid mixture which can and is to be separated by distillation; the process according to the invention may also be applied for distilling azeotropic mixtures, which is done with an auxiliary substance. The separation of lower boiling hydrocarbon mixtures, e. g., benzines, into narrow fractions, of mixtures of alcohols or of oleflnes, and like operations, may be advantageously effected according to the present process.

I claim:

1. The batch process for fractionating a quantity of a liquid distillable mixture containing a plurality of constituents of progressively different volatilities comprising confining said mixture in an unheated storage vessel, withdrawing a relatively small stream of said mixture from the storage vessel and introducing the same into an intermediate point of a distillation zone provided with dephlegmating and stripping sections, maintaining within the zone countercurrent streams of vapors and liquid reflux, simultaneously withdrawing top and bottom products from opposite ends of the zone and withdrawing at least a portion of the reflux from the dephlegmating section and from the distillation zone, introducing the withdrawn reflux into the storage vessel into contact with the remaining portion of the mixture and passing a relatively small stream of the resulting mixture to the said distillation zone, while withdrawing therefrom the said products and said portion of the reflux the only replenishment of distillable liquid for said tank being said withdrawn reflux.

2. The process of claim 1, in which the withdrawn reflux is first substantially cooled by an indirect heat exchange with the mixture passing from the storage vessel to the distillation zone and then introduced into the said vassel.

3. The batch process for fractionating a quantity of a liquid distillable mixture containing a plurality of constituents of progressively different volatiles comprising confining said mixture in an unheated storage vessel, withdrawing a relatively small stream of said mixture from the storage vessel and introducing the same into an intermediate point of a distillation zone provided with dephlegmating and stripping sections, maintaining within the zone countercurrent streams of vapors and liquid reflux, simultaneously withdrawing top and bottom products from opposite ends of the zone and withdrawing at least a portion of the reflux from the dephlegmatina section and from the distillation zone, introducing the withdrawn reflux into the storage vessel to commingle with the remaining portion of the mixture and passing a relatively small stream of the resulting mixture to the said distillation zone, while withdrawing therefrom the said products and said portion of the reflux the only replenishment of distillable liquid for said tank being said withdrawn reflux.

WILLEM J OHANNES DOMINICUS VAN DIJCK. 

